반응 #992697

반응 방정식

aniline

1-naphthoyl chloride

water

ammonium hydroxide

→

solid

수율 82.0%

Naphthalene-1-carboxylic acid phenylamide

수율 82.0%

용매

acetonitrile

diethyl ether

반응 조건

후처리

1. 1
   기타To the solution so formed
2. 2
   기타20 min
3. 3
   기타The phases were separated
4. 4
   세척the aqueous phase was washed with 100 ml of dichloromethane
5. 5
   기타The organic fractions were collected
6. 6
   건조dried with magnesium sulfate
7. 7
   여과filtered
8. 8
   기타the solvent was then removed under reduced pressure

실험 절차

4.77 g of 1-naphthoyl chloride (TCI America) was dissolved in 100 ml of anhydrous acetonitrile. To the solution so formed, 2.28 ml of aniline (Sigma-Aldrich) was added in a dropwise fashion over a period of c.a. 20 min. The reaction was then refluxed for 2 h at 82° C. 100 ml of distilled water and 5 ml of concentrated ammonium hydroxide were added along with 100 ml of diethyl ether in a separatory funnel. The phases were separated and the aqueous phase was washed with 100 ml of dichloromethane. The organic fractions were collected and dried with magnesium sulfate, filtered and the solvent was then removed under reduced pressure to yield a white solid 5.07 g (82%; 20.5 mmol).

출처